Teknologi Dan Rekayasa Kompetensi Keahlian Analisis Kimia

Analisis of Cemical Parameters SMK Negeri 13 Bandung

NITROGEN COMPOUND SMK Negeri 13 Bandung

Objectives After this session, the students are expected to be able : to explain the steps of determination of ammonium, nitrate and nitrite to explain the objectives of every step to explain the function of reagents to conduct the determination of ammonium, nitrate and nitrite to do the calculation in the determination of ammonium, nitrate and nitrite to arrange the report of the determination of ammonium, nitrate and nitrite Teknologi dan Rekayasa

Nitrogen Compound in water Ammonia (NH3) NH4+ appear at low pH Nitrogen gas (N2) Nitrite (NO2-) Nitrate (NO3-) NH4+ NH4+- Protein

Nitrogen Gas (N2) in water Presence of N2 in water produced from air, used by seaweed and groups of bacteria to growth N2 un reactiv N2 easy to get from water low level of saturation  Presence in water not harmful

Ammonia (NH3) in water Ammonia, at low pH  NH4+ (amonium), high pH  NH3 (ammonia) In surface water proceed against : - wastes of human (urine) - Microbiological decomposition of organic substances C,H,O,N,S + O2  CO2 + H2O + NH3 - Contamination of using fertilizer in agriculture Content of ammonia in surface water (30 mg/L) higher than groundwater Content ammonia in high level in water indicates high contamination (odor and taste) Condition for drinking water, NH3 must have 0 ppm, in river up to standard 0,5 ppm Removal process by aeration and chlorination

Determination of Ammonia (NH3) Determined as : - NH4+ (ammonium),dissolved in water - NH4+ - Protein, nitrogen compound formed as protein Method of determination by colorimetric with constant height, using Nessler and comparator Disrupt ion at analysis process : High level of Sulfide  add Zn(CH3COO)2, filtrate continued High level of Ca2+ and Mg2+  add caustic soda, filtrate continued Turbidity  add coagulant (tawas Al), filtrate continued

Determination of Ammonium (NH4+) Method of determination by colorimetric with constant height, using Nessler and comparator Reactant for colour formation Nessler Principle : NH4+ in water react to Nessler formed yellow-brown compound, compare the colour to standard solution Reactions : Nessler reactant : HgI2, KI, NaOH (K2HgI4) NH4+ + 2[HgI4]2- + 4OH-  HgO.Hg(HH2)I(s) + 7I- + 3H2O

Determination of Ammonium (NH4+) Making of stock NH4+ solution 100 ppm from NH4Cl Making of standard measurement 0,1 – 0,5 ppm In to Nessler tube Preparation of sample : Put 100 mL of sample (use graduated glass) in to Nessler tube (if there is disrupt must have losed before measurement) Add 1 mL Siegnette solution, shake it well and 1 mL Nessler reactant, shake in to sample and standard Let for 15 minutes, and compare the colour formed

Calculation (NH4+, mg/L) Method: colorimetric constant height (Nessler method)  Same intensity, same colour indicates same consentration According Lambert-Beer’s Law A1 = A2 1.b1.c1 = 2.b2.c2 b1= b2 ; 1 = 2  c1 = c2

Calculation (NH4+, mg/L) Method colorimetric with different height Same intensity,same colour indicates same concentration According Lambert-Beer’s Law A1 = A2 1.b1.c1 = 2.b2.c2 1= 2 , so : b1.c1 = b2.c2 if : 1 standard, 2 sample, so : b1.c1 c2 = b2

Determination of Ammonium-Protein (NH4+-Protein) Method of determination colorimetric constant height Reactant for colour formation is Nessler Principle : Protein in sample oxidized by K2S2O8 in acid condition to NH4+ salt, NH4+ through Nessler reactant formed yellow-brown compound ,compare the colour formation to standard solution Reactions : Nessler reactant : HgI2, KI, NaOH (K2HgI4) R-CNH2COOH + H+ + S2O82-  CO2 + H2O + (NH4)2SO4 NH4+(*) + 2[HgI4]2- + 4OH-  HgO.Hg(NH2)I(s) + 7I- + 3H2O

Determination of NH4+ Making of standard measurement 0,1 – 0,5 ppm In to nessler tube from stock solution 100 ppm Preparation of sample : Put 100 mL of sample in to Erlenmeyer flask Add H2SO4 4 N ( congo paper red  blue) Add 0,1g K2S2O8, heat for 15’ on steam bath Let it cool then put in to nessler tube add1 mL Siegnette solution shake it well and 1 mL Nessler reactant, shake in to sample and standard Let it for 15 minutes, compare the colour

Calculation NH4+-Protein, mg/L Method colorimetric different height  Same intensity of colour indicates same concentration According Lambert-Beer’s Law A1 = A2 1.b1.c1 = 2.b2.c2 1= 2 , so : b1.c1 = b2.c2 if 1 standar, 2 sample, so : b1.c1 c2 = b2

Calculation NH4+-Protein, mg/L When oxidizing proces, nitrogen in protein changed to NH4+ salt  then NH4+ which soluble increase from the process In order to detect consentration NH4+-Protein in water must corrected to free NH4+ dissolved in water NH4+-Protein = ppm NH4+(total) - ppm NH4+(free)

Nitrite (NO2-) in Water Nitrite : unstable (not long lasting )  temporary condition from oxidizing process NH4+ to NO3- (nitrification) 2NH4+ + 3 O2  2NO2- + 4H+ +2H2O + energy 2NO2- + O2  2 NO3- + energy Nitrite in water from inhibitor corrosive substances mostly used in manufacturer Nitrogen compound in formation of nitrite is the most harmful to human body cause : 1. React with hemoglobin on blood, until blood could not carry away oxygen 2. Formation of nitrosin (RR’N-NO)  carsinogenic

Determination of Nitrite (NO2-) Method of determination colorimetric constant height Reactant for colour formation: Griez-Romyn Principle : Nitrite in sample react with Griez-Romyn formed Red compound, compare the colour to standard solution Reaction : Diazotisation of sulfonil acid by nitrite acid, followed by coupling reaction wiht -naftilamina formed red dye azo

Determination of Nitrite (NO2-) Making of standard measurement 0,01 – 0,05 ppm in nessler tube from stock solution 100 ppm Preparation sample: Put 100 mL of sample in to nessler tube Add 100 mg nitrite reactant(Griez-Romyn), shake it well Let it for 10’  do simultaneously between sample and standard Compare the colour, under 30 minutes

Calculation (Nitrite, mg/L) Method determination colorimetric different height  Same intensity of colour indicates same consentration According Lambert-Beer’s Law A1 = A2 1.b1.c1 = 2.b2.c2 1= 2 , so : b1.c1 = b2.c2 If : 1 standard, 2 sample, so : b1.c1 c2 = b2

Nitrate (NO3-) in water Nitrite of nitrogen compound which has stable characteristic. In the water, it comes from : - Industrial banishment of explosive material, fertilizer, paint, etc. - The use of fertilizer in farming. The degree of nitrite in the water is not more than 10 ppm. The height of nitrite compound can cause : - the stimulation of algae and water plants growth which is unlimited -> if the level of DO is low means water animals are dead.

Nitrate (NO3-) in water - Metamoglobenia disease (cynose/blue disease which happens to babies). Nitrite is reduced by the bacterial of lactic acid in mother’s milk to become nitrite. Nitrite has a bond with the hemoglobin in the blood.

Determination of Nitrate (NO3-) Method of colorimetry of permanent height. Reactant of Nessler color shaper. Principle : Nitrate and nitrite in the sample is reduced by H2 from Al and NaOH to become NH4+ , NH4+ by nessler reactant which form yellow-brown substance, then the colour which is formed later is compared with the color standard solution.

Determination of Nitrate (NO3-) Reaction : 6NaOH + 2Al  3H2 + 2Na3AlO3 NO2- + 3H2  NH3 +OH- + H2O NO3- + 4H2  NH3 + OH- + 2H2O NH4+ + 2[HgI4]2- + 4OH-  HgO.Hg(NH2)I(s) + 7I- + 3H2O

Determination of Nitrate (NO3-) The make of measurement standard of NH4 + 0,1 – 0,5 ppm In nessler tube from stock solution 100 ppm Sample preparation : Put 100 mL to erlenmeyer flask Add 25 % of NaOH solution and Al metal, save it for 1 night The gas is put in 0,01 N of HCl solution Put into nessler tube Add 1 mL of Siegnette solution. And then shake. After that add 1 mL of nessler reactant to the sample and standard Save it for 15 minutes, and compare the color which Happens later

Calculation (Nitrate, mg/L) Method : Colorimetry the height changes  Intensity of the same colour shows the same concentration According to Lambert-Beer law A1 = A2 1.b1.c1 = 2.b2.c2 1= 2 , maka : b1.c1 = b2.c2 If : 1 standard, 2 sample, so : b1.c1 c2 = b2

Calculation (Nitrate, mg/L ) When the reduction happens, nitrate and nitrite in the sample is changed into NH4 +  so NH4 + measured becomes total ammonium of nitrite, nitrate and free ammonium. So, to count the nitrate concentration in the water has to be corrected to free NH4 + and nitrite. NH4+ from NO3- = NH4+(total) - NH4+dari NO2- - NH4+(free) Mr. NH4+ ppm NH4+from NO2- = x ppm NO2- Mr. NO2- Mr. NO3- Ppm NO3- = x ppm NH4+ dari NO3- Mr. NH4+